CN110504491A - Method for modifying all-solid-state lithium battery by modified succinonitrile - Google Patents

Method for modifying all-solid-state lithium battery by modified succinonitrile Download PDF

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Publication number
CN110504491A
CN110504491A CN201910802415.3A CN201910802415A CN110504491A CN 110504491 A CN110504491 A CN 110504491A CN 201910802415 A CN201910802415 A CN 201910802415A CN 110504491 A CN110504491 A CN 110504491A
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succinonitrile
solid
modified
lithium battery
garnet
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CN110504491B (en
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刘芳洋
赖延清
徐向群
汪齐
蒋良兴
贾明
李劼
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Hunan Enjie Frontier New Material Technology Co ltd
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Central South University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/056Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562Solid materials
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/058Construction or manufacture
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00Electrolytes
    • H01M2300/0017Non-aqueous electrolytes
    • H01M2300/0065Solid electrolytes
    • H01M2300/0068Solid electrolytes inorganic
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a method for modifying an all-solid-state lithium battery by modified succinonitrile, wherein a modification layer is arranged between a solid electrolyte layer and a negative electrode of the all-solid-state lithium battery, the modification layer is modified succinonitrile with the thickness of 10nm-100 mu m, the modified succinonitrile comprises succinonitrile, garnet type electrolyte powder and an additive, and the preparation step of the modified succinonitrile comprises the following steps: according to the weight ratio of (49.9-80) to (10-50): (0.1-10) weighing succinonitrile, garnet electrolyte powder and additive in a mass ratio, and heating and stirring the succinonitrile, the garnet electrolyte powder and the additive uniformly; and coating the stirred solution on the solid electrolyte layer and/or the negative electrode, and standing and solidifying to obtain the modification layer. The modification layer can form a good lithium ion channel between the negative electrode and the solid electrolyte; the added garnet electrolyte powder can avoid the problem that lithium salt is added to seriously absorb water in the air; the all-solid-state battery structure prepared by the invention and the added additive can greatly reduce the interface impedance.

Description

The method of modified succinonitrile modification solid lithium battery
Technical field
The present invention relates to solid lithium battery fields, and in particular to a kind of side of modified succinonitrile modification solid lithium battery Method.
Background technique
In the case where bringing environmental pollution and greenhouse effects using traditional energy, new energy is in the every aspect of life Play increasingly important role.Lithium ion battery is special with long-term cyclical stability, environmental-friendly and life time length etc. Point is widely applied in energy storage field, but on the one hand present lithium ion battery is unable to satisfy growing energy density and needs It asks, another aspect lithium ion battery itself causes explosion danger seriously to limit further development using flammable electrolyte. Therefore it is necessary for developing using solid lithium battery, and solid electrolyte is non-combustible, and electrochemical window mouth width can match lithium simultaneously Cathode and high pressure cobalt acid lithium and ternary material, the energy density of significant increase battery.
It is on the other hand that cathode of lithium has very by force but on the one hand since solid electrolyte and cathode of lithium belong to affixed touching Reproducibility and solid electrolyte middle high-valence state metal cation occur reduction reaction generate high impedance interface phase, solid-state electricity Showing on long-term cyclical stability and high rate performance for pond is poor.
Summary of the invention
The present invention, which essentially consists in, provides a kind of preparation method of modified succinonitrile modification solid lithium battery cathode, mainly Solve existing method be unable to improve all-solid-state battery long-term cycle stability and poor high rate performance.
To achieve the goals above, the method for a kind of modified succinonitrile modification solid lithium battery provided by the invention, institute Stating solid lithium battery includes anode, solid-state electrolyte layer, decorative layer and cathode, and the solid-state electrolyte layer is between the anode Between the decorative layer, for the decorative layer between solid-state electrolyte layer and cathode, the decorative layer is modified succinonitrile, described Modified succinonitrile includes succinonitrile, Garnet-type electrolyte powder and additive, and the decorative layer is with a thickness of 10nm-100 μm, The preparation step of the modified succinonitrile includes:
Step 1: press (49.9-80): (10-50): (0.1-10) mass ratio weighs succinonitrile, Garnet-type electrolyte powder End and additive, three's heating stirring is uniform;
Step 2: by solution spraying that step 1 obtains or being spin-coated on solid-state electrolyte layer and/or cathode, stand solidification After obtain decorative layer.
Preferably, the granular size of Garnet-type electrolyte powder is 5nm-50 μm in step 1.
Preferably, the heating temperature in step 1 is 50-90 DEG C, heating time 1-36h.
Preferably, the chemical general formula of the Garnet-type electrolyte is Li7-3x+y-zAxLa3-yByZr2-zCzO12, wherein A packet Include one of Ga or Al or a variety of;B includes one of Ca, Sr, Ba or Ce or a variety of;C include Ta, Nb, Ge, Sc, W, Zr, One of Hf, Sn or Sb or a variety of, x, y, z indicate molar ratio, 0≤x≤0.3,0≤y≤2,0≤z≤0.2.
Preferably, the additive is the one or more of FEC, lithium nitrate, lithium nitrite and copper fluoride.
Technical concept of the invention is as follows:
Sun et al. (Adv.Funct.Mater.2019,1900392) use lithium salts to be dissolved in succinonitrile after as cathode interface Decorative layer, improvement interface problem that can be very big improve chemical property, but this is dissolved in the operation needs of succinonitrile due to lithium salts It operates under an inert atmosphere, increases production cost, in addition succinonitrile film forming itself is very poor, and can not effectively inhibit lithium branch Brilliant growth.And carbuncle type powder mixing succinonitrile is used, and certain additive is cooperated to can effectively improve to the quick of air Perception and film forming.
Compared to the prior art, the present invention has at least the following advantages:
(1) modification succinonitrile of the invention is plastic crystal electrolyte, using plastic crystal electrolyte as decorative layer, just due to itself It is a kind of excellent lithium ion conductor, good lithium ion tunnel can be formed between cathode and solid electrolyte.
(2) the Garnet-type electrolyte powder being added can operate in air, be avoided that lithium salts is added to be inhaled in air The serious problem of water.
(3) all-solid-state battery structure prepared by the present invention and the additive of addition can effectively inhibit negative electrode material and solid Interfacial reaction and high valence elements between electrolyte restore problem, greatly reduction interface impedance.
(4) method and process for preparing all-solid-state battery of the invention is simple, can be mass-produced.
Detailed description of the invention
Fig. 1 is the ionic conductance by the way that the plastic crystal electrolyte that the Garnet-type electrolyte powder of different content measures is added Rate.
Fig. 2 is the constant-current discharge performance curve for the all-solid-state battery that embodiment 1 obtains.
Specific embodiment
Below by embodiment, the present invention is further illustrated, but not limited to this.
Embodiment 1
Choose LiFeO4As positive electrode Tu Bucheng pole piece, the Li of NASICON type1.4Al0.4Ti1.6(PO4)3As electrolysis The thin slice that matter is pressed into 13mm is sintered, and lithium metal is as cathode.According to different ratio 10-60% carbuncle type powder Li7La3Zr2O12(LLZO) mixing adds in succinonitrile, and 10% FEC is added as additive, and uniform stirring is for 24 hours at 70 DEG C.Fig. 1 The ionic conductivity obtained at different temperatures for the plastic crystal electrolyte of the Garnet-type electrolyte powder of different proportion obtained (25℃,40℃,50℃,60℃).From fig. 1, it can be seen that the plastic crystal electrolyte of the Garnet-type electrolyte powder of 20% mass fraction Ionic conductivity at each temperature is generally optimal.
The plastic crystal product for choosing the LLZO doping of 20% mass fraction is spin-coated on solid electrolyte sheet, stands solidification Afterwards, the decorative layer of 4 μ m-thicks is made.It is suitable according to anode-electrolyte-decorative layer-cathode using full battery manufactured in the present embodiment Sequence is assembled into button cell and is tested.When at 25 DEG C with the 0.2C constant-current discharge of positive electrode, 60 circle specific capacity of circulation still may be used It is maintained at 134mAh/g, shows good cycle performance.
Embodiment 2
Choose LiCo0.8 Ni0.1Al0.1O2As positive electrode Tu Bucheng pole piece, the Li of NASICON type1.4Al0.4Ti1.6 (PO4)3The thin slice for being pressed into 20mm as electrolyte is sintered, and lithium metal is as cathode.According to 60:40:5 weigh succinonitrile, Carbuncle type powder Li7La3Zr2O12(LLZO) and lithium nitrate, at 80 DEG C after uniform stirring 12h, plastic crystal product obtained is revolved It is coated on solid electrolyte sheet, after standing solidification, the decorative layer of 20 μ m-thicks is made.It is pressed using full battery manufactured in the present embodiment It is assembled into button cell according to anode-electrolyte-decorative layer-cathode sequence and is tested.With the 0.2C of positive electrode at 25 DEG C When constant-current discharge, 60 circle specific capacity of circulation may remain in 130mAh/g, show good cycle performance.

Claims (5)

1. a kind of method of modified succinonitrile modification solid lithium battery, which is characterized in that the solid lithium battery includes just Pole, solid-state electrolyte layer, decorative layer and cathode, the solid-state electrolyte layer is between the anode and the decorative layer, institute Decorative layer is stated between solid-state electrolyte layer and cathode, the decorative layer is modified succinonitrile, and the modified succinonitrile includes fourth two Nitrile, Garnet-type electrolyte powder and additive, and the decorative layer is with a thickness of 10nm-100 μm, the system of the modified succinonitrile Include: for step
Step 1: press (49.9-80): (10-50): (0.1-10) mass ratio weigh succinonitrile, Garnet-type electrolyte powder and Additive, three's heating stirring is uniform;
Step 2: by solution spraying that step 1 obtains or being spin-coated on solid-state electrolyte layer and/or cathode, stand after solidification To decorative layer.
2. the method for modified succinonitrile modification solid lithium battery according to claim 1, which is characterized in that in step 1 The granular size of Garnet-type electrolyte powder is 5nm-50 μm.
3. the method for modified succinonitrile modification solid lithium battery according to claim 1, which is characterized in that in step 1 Heating temperature be 50-90 DEG C, heating time 1-36h.
4. the method for modified succinonitrile modification solid lithium battery according to claim 1, which is characterized in that the pomegranate The chemical general formula of stone-type electrolyte is Li7-3x+y-zAxLa3-yByZr2-zCzO12, wherein A includes one of Ga or Al or a variety of;B Including one of Ca, Sr, Ba or Ce or a variety of;C includes one of Ta, Nb, Ge, Sc, W, Zr, Hf, Sn or Sb or a variety of, X, y, z indicates molar ratio, 0≤x≤0.3,0≤y≤2,0≤z≤0.2.
5. the method for modified succinonitrile modification solid lithium battery according to claim 1, which is characterized in that the addition Agent is the one or more of FEC, lithium nitrate, lithium nitrite and copper fluoride.
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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN111509195A (en) * 2020-05-07 2020-08-07 武汉理工大学 Surface modification method for metal lithium cathode in all-solid-state lithium battery
CN112563568A (en) * 2020-11-13 2021-03-26 上海空间电源研究所 Preparation method of all-solid-state battery interface layer and all-solid-state battery
CN112993383A (en) * 2019-12-18 2021-06-18 财团法人工业技术研究院 Battery with a battery cell
CN113036131A (en) * 2019-12-09 2021-06-25 财团法人工业技术研究院 Positive electrode material, positive electrode containing same, and battery
CN113258172A (en) * 2021-04-19 2021-08-13 中国科学院青岛生物能源与过程研究所 Solid electrolyte suitable for room-temperature all-solid-state zinc-air battery and preparation method thereof
WO2021225248A1 (en) * 2020-05-06 2021-11-11 주식회사 엘지에너지솔루션 Method for manufacturing secondary battery having improved resistance
CN114497719A (en) * 2021-12-31 2022-05-13 中南大学 Interface connecting layer of solid-state battery and preparation method thereof
CN114759269A (en) * 2022-05-18 2022-07-15 电子科技大学 Integrated all-solid-state battery based on ceramic-based electrolyte sheet and preparation method
CN115498255A (en) * 2022-09-20 2022-12-20 电子科技大学 Method for improving composite solid electrolyte interface in situ

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113036131A (en) * 2019-12-09 2021-06-25 财团法人工业技术研究院 Positive electrode material, positive electrode containing same, and battery
CN112993383A (en) * 2019-12-18 2021-06-18 财团法人工业技术研究院 Battery with a battery cell
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WO2021225248A1 (en) * 2020-05-06 2021-11-11 주식회사 엘지에너지솔루션 Method for manufacturing secondary battery having improved resistance
CN111509195A (en) * 2020-05-07 2020-08-07 武汉理工大学 Surface modification method for metal lithium cathode in all-solid-state lithium battery
CN112563568A (en) * 2020-11-13 2021-03-26 上海空间电源研究所 Preparation method of all-solid-state battery interface layer and all-solid-state battery
CN113258172A (en) * 2021-04-19 2021-08-13 中国科学院青岛生物能源与过程研究所 Solid electrolyte suitable for room-temperature all-solid-state zinc-air battery and preparation method thereof
CN114497719A (en) * 2021-12-31 2022-05-13 中南大学 Interface connecting layer of solid-state battery and preparation method thereof
CN114759269A (en) * 2022-05-18 2022-07-15 电子科技大学 Integrated all-solid-state battery based on ceramic-based electrolyte sheet and preparation method
CN115498255A (en) * 2022-09-20 2022-12-20 电子科技大学 Method for improving composite solid electrolyte interface in situ

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